Mo5Si3-20%Al2O3 （mass fraction） nanocomposite was synthesized by mechanical alloying （MA） of mixture of MoO3,Mo,Si and Al powders.The structural evolutions of powder particles during mechanical alloying were studied by X-ray diffractometry （XRD）,scanning electron microscopy （SEM）,transmission electron microscopy （TEM） and differential thermal analysis （DTA）.Results show that Mo5Si3-20%Al2O3 was obtained after 10 h of milling.The spontaneous reaction of powders takes place in an explosive mode.The crystallite sizes of Mo5Si3 and Al2O3 after milling for 30 h were 36.3 nm and 21.9 nm,respectively.With longer milling time,the intensities of Mo5Si3 and Al2O3 peaks decreased and became broad due to the decrease in crystallite size.Thermal analysis results and XRD analysis results show that the Mo5Si3-Al2O3 nanocomposite powders are very stable during milling （up to 30 h） and heating （up to 1 000℃） and no transformation takes place.
